反应详情

2,4-bis-benzyloxy-5-isopropyl-N-[4-(morpholin-4-yl)-phenyl]-benzene-carbohydrazonamide (F370-IM4: crude product) was suspended in tetrahydrofuran (10 mL), mixed with 1,1′-carbonyldiimidazole (1.12 g, 6.9 mmol) and the mixture was stirred at room temperature for 2 hours. The reaction mixture was partitioned between ethyl acetate (50 mL) and 5% aqueous sodium hydrogencarbonate (50 mL), and the organic layer was separated. The organic layer obtained was dried over anhydrous sodium sulfate. Sodium sulfate was removed by filtration, and the solvent was distilled off under reduced pressure, and the residue thus obtained was purified by silica gel column chromatography (ethyl acetate 100%). The obtained product was purified by suspending in ethyl acetate to obtain the title compound (F370-IM5: white crystals, 1.2 g, 45% in 3 steps).

1. customThe reaction mixture was partitioned between ethyl acetate (50 mL) and 5% aqueous sodium hydrogencarbonate (50 mL)
2. customthe organic layer was separated
3. customThe organic layer obtained
4. dry with materialwas dried over anhydrous sodium sulfate
5. customSodium sulfate was removed by filtration
6. distillationthe solvent was distilled off under reduced pressure
7. customthe residue thus obtained
8. customwas purified by silica gel column chromatography (ethyl acetate 100%)
9. customThe obtained product was purified